Chemical Monitoring On Site (CM Onsite) organised by NORMAN Association and JRC in support of CIS WFD NORMAN Interlaboratory study (ILS) on passive sampling of emerging pollutants Branislav Vrana Water Research Institute, Slovakia

Activities of NORMAN network in passive sampling  An expert group meeting in 2009  A position paper “Passive sampling of emerging pollutants in the aquatic environment: state of the art and perspectives” in 2010  An interlaboratory calibration study in

Interlaboratory calibration study in 2011 present variability in data by comparing results from various passive samplers sent by participating laboratories exposed to water at a single (reference) site Target substances: –polar pesticides - 19 participants –Pharmaceuticals – 17 participants –steroid hormones – 15 participants –Triclosan - 8 participants –bisphenol A - 11 participants –PFOA, PFOS - 8 participants –PBDE -16 participants 30 participants from commercial, academic and regulatory laboratories Silicone strips CONTACT:

Interlaboratory study DESIGN a sampler comparison exercise extended to cover individual aspects in the passive sampling process –analytical comparability –comparison with spot sampling

Study design 1. Passive samplers from participants Coordinator Participant 1 Participant 2 Participant 3 Participant 4 Sampler 3 Sampler 2 Sampler 1 for selected analyte/analytes Sampling site - sampler exposure Sampler 1Sampler 2 Sampler 3Sampler 4 Quasimeme Report to database ng/sampler of compound A ng/cm 2 sampler of compound A ng/L water of compound A calculation procedure for compound A

Study design 2. Standard solution Coordinator Participant 1 Participant 2 Participant 3 Participant 4 send to coordinator Central laboratory S Standard solution S SS S purchase standard prepare a QC solution prepare multiple vials (according to participant registration) check homogeneity send to coordinator S S S S distribute standards for selected analyte/analytes Quasimeme Report to database ng/ml of substance A

Study design 3. Provided passive samplers Coordinator Participant 1 Participant 2 Participant 3 Participant 4 for selected analyte/analytes Sampling site - sampler exposure Provided sampler Provided sampler Provided sampler Provided sampler Buy or prepare Provided sampler Provided sampler Provided sampler Provided sampler Provided sampler Provided sampler Provided sampler Provided sampler Central laboratory Provided sampler 3. Quasimeme Report to database ng/sampler of compound A ng/cm 2 sampler of compound A ng/L water of compound A calculation procedure Report to database ng/sampler of compound A ng/cm 2 sampler of compound A ng/L water of compound A calculation procedure

Study design 4. Water samples Coordinator for selected analyte/analytes Sampling site - sampler exposure Central laboratory W water sample W W W W W W analyse water samples collect water sample send to central laboratory Provided sampler Sampler 3 Sampler 2 Sampler 1 Sampler 4 Provided sampler Provided sampler Provided sampler Quasimeme Report to database ng/L water of compound A NOT APPLICABLE FOR HYDROPHOBIC COMPOUNDS PBDE…

Interlaboratory study Steering group RoleOrganisationActivity CoordinatorVUVH Slovakia coordination, sampling activities, logistics Central laboratory for pesticides Cemagref Bordeaux France Preparation of QC standards, analysis of provided samplers analysis of water samples Central laboratory for pharmaceuticals ISM-LPTC, University of Bordeaux, France Preparation of QC standards, analysis of provided samplers analysis of water samples Central laboratory for Steroid hormones Cemagref Lyon France Preparation of QC standards, analysis of provided samplers analysis of water samples Central laboratory for PFOSDG JRC IES Preparation of QC standards, analysis of provided samplers analysis of water samples Central laboratory for BDERECETOX + DELTARES Preparation of QC standards, analysis of provided samplers NO analysis of water

Interlaboratory study Steering group RoleOrganisationActivity Central laboratory for bisphenol A, triclosan UK Environment Agency Preparation of QC standards, analysis of provided samplers analysis of water samples Sampling supportInsitute of Public Health Ostrava, Czech Republic Support at the sampling site Sampling support Data interpretation RECETOX, Masaryk University, Czech rep. Support at the sampling site Participant registration Data interpretation, report preparation Participant interface for uploading results Data-assessment and Reporting results QUASIMEME Setup of the experiment into a database Setup of sharepointsites Instruction of laboratories how to get access to the sharepointsite Introduce the lab specific contact information into the database. Do the data-assessment Produce figures and excel sheets of the assessed data. Produce z-score lists for each individual laboratory. Help desk facility with respect to data- transfer

Target compounds Pesticides and their degradation products: Terbutylazine Desethylatrazine Desethylterbutylazine Atrazine Carbendazim S-metolachlor Diuron Pharmaceuticals: Carbamazepine Diclofenac Ibuprofen Naproxen Diazepam Alprazolam Ketoprofen Atenolol Steroid hormones: 17-alpha-Estradiol 17-alpha-Ethinylestradiol 17-beta-Estradiol Estriol Estrone Bisphenol A Triclosan Brominated flame retardants BDE 28, 47, 99, 100, 153 and 154 Fluorinated surfactants PFOA, PFOS

Campaign timing: passive sampler deployment Campaign number Class number Compound class Registration deadline Deadline for sending samplers + deployment equipment Sampler exposure Sampler deployment period 11Pesticides days Pharmaceutic als 23 Steroid hormones days PFOA PFOS 5 Bisfenol A, Triclosan 36PBDE days

Continuous water sampling

Sampler preparation for deployment

Sampler deployment

Sampler recovery

Onsite sampler cleaning and preparation

Laboratory preparation of provided samplers

Dissemination of results 3 rounds, May-August – a workshop will be organised to disseminate results.

Study results Statistics: 30 participating laboratories from Europe, North America and Australia 292 reference samplers for polar compounds distributed 80 reference samplers for PBDE 268 participant samplers for pesticides and pharmaceuticals 285 participant samplers for PFOS, steroids, bisphenol A and triclosan 132 participant samplers for PBDE Total: cca samplers were deployed at the reference site and distributed for analysis The reporting deadline for laboratories has been set to 15 th December A dissemination workshop will be organised in 2012 organised by NORMAN + DG JRC